固相膜萃取-超声洗脱衍生法分析水中酚类化合物
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摘要
建立了水中酚类化合物的新型预处理技术。在水样pH 3~4时,采用SDB-XC固相萃取膜,5min可完成500mL水样中酚类化合物的萃取;将膜片折叠置于反应瓶中,以五氟苄基溴溶液为衍生试剂,20min可完成膜片上酚类化合物的超声洗脱和衍生;以HP-5MS色谱柱(30m×0.25mm×0.25μm)为分析柱,用负化学电离源在10min内完成检测。对膜片的选择、酸度的控制、衍生条件、超声条件及干扰情况进行逐一分析并优化,结果表明,在10~200μg/L线性范围内,各组分的相关系数r2>0.997,加标回收率在70%~107%之间,相对标准偏差为3.8%~10.4%。应用该方法检测实际样品,部分样品有检出。该方法可实现样品的快速萃取、洗脱衍生一体化、低污染和高灵敏检测。
A new pretreatment technology of phenolic compounds analysis in water was established.When the pH value of the water sample was 3-4,the extraction of phenolic compounds in 500 mL water sample could be completed in 5 min by using SDB-XC solid phase extraction membrane.Then the folded membrane was put into a reaction bottle,in which five fluorinated benzyl bromide solution was used as the derivatization reagent to complete the elution and derivatization of phenolic compounds on the membrane by20 min ultrasound.HP-5 MS column(30 m×0.25 mm×0.25μm)was selected as analytical column,the detection could be completed within 10 min by using negative chemical ionization source.In this method,the selection of membrane,the control of acidity,derivation condition,ultrasonic condition and interference situation were analyzed and optimized.The results showed that the correlation coefficient of each component was greater than 0.997 in the linear range of 10-200μg/L.The recoveries of different concentrations were 70%-107%,and the relative standard deviations were 3.8%-10.4%.Some phenolic compounds were detected in actual samples by this method.The method can achieve the rapid extraction,synchronous elution,low pollution and high sensitivity detection of samples.
A new pretreatment technology of phenolic compounds analysis in water was established.When the pH value of the water sample was 3-4,the extraction of phenolic compounds in 500 mL water sample could be completed in 5 min by using SDB-XC solid phase extraction membrane.Then the folded membrane was put into a reaction bottle,in which five fluorinated benzyl bromide solution was used as the derivatization reagent to complete the elution and derivatization of phenolic compounds on the membrane by20 min ultrasound.HP-5 MS column(30 m×0.25 mm×0.25μm)was selected as analytical column,the detection could be completed within 10 min by using negative chemical ionization source.In this method,the selection of membrane,the control of acidity,derivation condition,ultrasonic condition and interference situation were analyzed and optimized.The results showed that the correlation coefficient of each component was greater than 0.997 in the linear range of 10-200μg/L.The recoveries of different concentrations were 70%-107%,and the relative standard deviations were 3.8%-10.4%.Some phenolic compounds were detected in actual samples by this method.The method can achieve the rapid extraction,synchronous elution,low pollution and high sensitivity detection of samples.
引文
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[9]杨丽莉,王美飞,胡恩宇,等.超声波提取-气相色谱法测定土壤中21种酚类化合物[J].色谱,2013,31(11):1 081-1 086.YANG Lili,WANG Meifei,HU Enyu,et al.Determination of 21phenolic compounds in soft by ultrasonic extraction-gas chromatography[J].Chinese Journal of Chromatography,2013,31(11):1 081-1 086(in Chinese).
[10]潘海祥,麦碧娴,庄汉平,等.使用C18固相萃取膜-色质联用定量分析饮用水中痕量多环芳烃的初步研究[J].分析化学,1999,27(2):140-144.PAN Haixiang,MAI Bixian,ZHUANG Hanping,et al.Quantitative analysis of trace polycyclic aromatic hydrocarbons in drinking water with C18-solid-phase extraction-gas chromatography/mMass spectrometry[J].Chinese Journal of Analytical Chemistry,1999,27(2):140-144(in Chinese).
[11]张莉,桂建业,赵国兴,等.固相膜萃取-超声洗脱-原位衍生法分析水中不同极性农药残留[J].分析化学,2014,42(4):592-596.ZHANG Li,GUI Jianye,ZHAO Guoxing,et al.Determination of different polarity pesticide residues in water by solid phase membrane extraction-ultrasonic assisted elution-in situ derivatization method[J].Chinese Journal of Analytical Chemistry,2014,42(4):592-596(in Chinese).
[2]HJ 744—2015.水质酚类化合物的测定气相色谱-质谱法[S].北京:中国环境科学出版社,2015.
[3]SL463—2009.气相色谱酚测定水中酚类化合物[S].北京:水利水电出版社,2010.
[4]苏宇亮,胡克武.水中酚类化合物的固相萃取-气质联用法测定[J].分析测试学报,2008,27(增刊1):127-129.SU Yuliang,HU Kewu.Determination of phenols in water by solid phase extraction and gas chromatography-mass spectrometry[J].Journal of Instrumental Analysis,2008,27(Suppl 1):127-129(in Chinese).
[5]任雪东,吕蓉,刘成雁,等.水中11种酚类化合物的固相萃取/气相色谱-质谱/选择离子法测定[J].分析测试学报,2008,27(5):501-504.REN Xuedong,LV Rong,LIU Chengyan,et al.Determination of 11phenolic compounds in water by solid phase extraction/gas chromatographymass spectrometry with selected ion monitoring mode[J].Journal of Instrumental Analysis,2008,27(5):501-504(in Chinese).
[6]U.S.EPA Method 3550B,Ultrasonic extraction[S].Washington,DC:U.S Government Printing Office,1996.
[7]HJ911—2017.土壤和沉积物有机物的提取超声波萃取法[S].北京:中国环境科学出版社,2018.
[8]张莉,桂建业,张辰凌,等.原位衍生分析土壤中多种酸性有机农药残留[J].质谱学报,2015,36(2):135-140.ZHANG Li,GUI Jianye,ZHANG Chenling,et al.In situ derivatization analysis of acidic organic pesticide residues in soil[J].Journal of Chinese Mass Spectrometry Society,2015,36(2):135-140(in Chinese).
[9]杨丽莉,王美飞,胡恩宇,等.超声波提取-气相色谱法测定土壤中21种酚类化合物[J].色谱,2013,31(11):1 081-1 086.YANG Lili,WANG Meifei,HU Enyu,et al.Determination of 21phenolic compounds in soft by ultrasonic extraction-gas chromatography[J].Chinese Journal of Chromatography,2013,31(11):1 081-1 086(in Chinese).
[10]潘海祥,麦碧娴,庄汉平,等.使用C18固相萃取膜-色质联用定量分析饮用水中痕量多环芳烃的初步研究[J].分析化学,1999,27(2):140-144.PAN Haixiang,MAI Bixian,ZHUANG Hanping,et al.Quantitative analysis of trace polycyclic aromatic hydrocarbons in drinking water with C18-solid-phase extraction-gas chromatography/mMass spectrometry[J].Chinese Journal of Analytical Chemistry,1999,27(2):140-144(in Chinese).
[11]张莉,桂建业,赵国兴,等.固相膜萃取-超声洗脱-原位衍生法分析水中不同极性农药残留[J].分析化学,2014,42(4):592-596.ZHANG Li,GUI Jianye,ZHAO Guoxing,et al.Determination of different polarity pesticide residues in water by solid phase membrane extraction-ultrasonic assisted elution-in situ derivatization method[J].Chinese Journal of Analytical Chemistry,2014,42(4):592-596(in Chinese).